RU2009107006A - METHOD FOR SEALING POROUS PRODUCTS - Google Patents

METHOD FOR SEALING POROUS PRODUCTS Download PDF

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RU2009107006A
RU2009107006A RU2009107006/03A RU2009107006A RU2009107006A RU 2009107006 A RU2009107006 A RU 2009107006A RU 2009107006/03 A RU2009107006/03 A RU 2009107006/03A RU 2009107006 A RU2009107006 A RU 2009107006A RU 2009107006 A RU2009107006 A RU 2009107006A
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starting material
liquid starting
porous substrate
reaction chamber
compaction
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RU2431628C2 (en
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Кенни ЧАН (US)
Кенни ЧАН
Брюс ЦИММЕРМАН (US)
Брюс ЦИММЕРМАН
Арно ФИЙОН (US)
Арно ФИЙОН
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Мессье-Бугатти (Fr)
Мессье-Бугатти
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Abstract

1. Способ уплотнения пористого субстрата, включающий: ! погружение пористого субстрата, находящегося в реакционной камере, в жидкое исходное вещество таким образом, что жидкое исходное вещество заполняет поры пористого субстрата; и ! индуктивный нагрев погруженного пористого субстрата до температуры, достаточной для пиролиза жидкого исходного вещества, с образованием продукта разложения, который осаждается внутри пор субстрата, в результате чего происходит уплотнение пористого субстрата, ! в котором степень химической чистоты жидкого исходного вещества регулируют таким образом, что она является ниже химически чистой, но достаточно химически чистой для получения продукта разложения, обладающего желаемыми физическими характеристиками. ! 2. Способ по п.1, в котором жидкое исходное вещество включает углеводород. ! 3. Способ по п.1, в котором продукт разложения включает углерод. ! 4. Способ по п.2, в котором углеводород выбран из группы, состоящей из циклопентана, циклогексена, 1-гексена, газолина, толуола, метилциклогексана, н-гексана, керосина, гидродесульфированного керосина, бензола и комбинаций указанных веществ. ! 5. Способ по п.1, в котором степень химической чистоты жидкого исходного вещества регулируют таким образом, что она составляет приблизительно от 80 до 99,9%. ! 6. Способ по п.5, в котором в жидком исходном веществе присутствуют примеси, и при этом примеси включают одно или более из следующих веществ: циклопентадиен, гексан, метилциклопентан, бензол, циклогексен, гептан, метилциклогексан, толуол, этилбензол, фенилацетилен, стирол, нонан, инден, нафталин, метилнафталин, аценафталин и флуорен. ! 7. Способ по пп.1-6 1. A method of densifying a porous substrate, comprising:! immersing the porous substrate in the reaction chamber in the liquid starting material so that the liquid starting material fills the pores of the porous substrate; and! inductive heating of the immersed porous substrate to a temperature sufficient for pyrolysis of the liquid starting material, with the formation of a decomposition product that precipitates inside the pores of the substrate, resulting in the compaction of the porous substrate,! in which the degree of chemical purity of the liquid starting material is controlled in such a way that it is lower than chemically pure, but sufficiently chemically pure to obtain a decomposition product having the desired physical characteristics. ! 2. The method according to claim 1, wherein the liquid starting material comprises a hydrocarbon. ! 3. The method according to claim 1, in which the decomposition product includes carbon. ! 4. The method according to claim 2, in which the hydrocarbon is selected from the group consisting of cyclopentane, cyclohexene, 1-hexene, gasoline, toluene, methylcyclohexane, n-hexane, kerosene, hydrodesulfurized kerosene, benzene, and combinations of these substances. ! 5. The method according to claim 1, in which the degree of chemical purity of the liquid starting substance is regulated so that it is from about 80 to 99.9%. ! 6. The method according to claim 5, in which impurities are present in the liquid starting material, and the impurities include one or more of the following substances: cyclopentadiene, hexane, methylcyclopentane, benzene, cyclohexene, heptane, methylcyclohexane, toluene, ethylbenzene, phenylacetylene, styrene , nonane, indene, naphthalene, methylnaphthalene, acenaphthalene and fluorene. ! 7. The method according to claims 1-6

Claims (17)

1. Способ уплотнения пористого субстрата, включающий:1. The method of compaction of a porous substrate, including: погружение пористого субстрата, находящегося в реакционной камере, в жидкое исходное вещество таким образом, что жидкое исходное вещество заполняет поры пористого субстрата; иimmersing the porous substrate in the reaction chamber in the liquid starting material so that the liquid starting material fills the pores of the porous substrate; and индуктивный нагрев погруженного пористого субстрата до температуры, достаточной для пиролиза жидкого исходного вещества, с образованием продукта разложения, который осаждается внутри пор субстрата, в результате чего происходит уплотнение пористого субстрата,inductive heating of the immersed porous substrate to a temperature sufficient for pyrolysis of the liquid starting material, with the formation of a decomposition product that precipitates inside the pores of the substrate, resulting in the compaction of the porous substrate, в котором степень химической чистоты жидкого исходного вещества регулируют таким образом, что она является ниже химически чистой, но достаточно химически чистой для получения продукта разложения, обладающего желаемыми физическими характеристиками.in which the degree of chemical purity of the liquid starting material is controlled in such a way that it is lower than chemically pure, but sufficiently chemically pure to obtain a decomposition product having the desired physical characteristics. 2. Способ по п.1, в котором жидкое исходное вещество включает углеводород.2. The method according to claim 1, wherein the liquid starting material comprises a hydrocarbon. 3. Способ по п.1, в котором продукт разложения включает углерод.3. The method according to claim 1, in which the decomposition product includes carbon. 4. Способ по п.2, в котором углеводород выбран из группы, состоящей из циклопентана, циклогексена, 1-гексена, газолина, толуола, метилциклогексана, н-гексана, керосина, гидродесульфированного керосина, бензола и комбинаций указанных веществ.4. The method according to claim 2, in which the hydrocarbon is selected from the group consisting of cyclopentane, cyclohexene, 1-hexene, gasoline, toluene, methylcyclohexane, n-hexane, kerosene, hydrodesulfurized kerosene, benzene, and combinations of these substances. 5. Способ по п.1, в котором степень химической чистоты жидкого исходного вещества регулируют таким образом, что она составляет приблизительно от 80 до 99,9%.5. The method according to claim 1, in which the degree of chemical purity of the liquid starting substance is controlled so that it is from about 80 to 99.9%. 6. Способ по п.5, в котором в жидком исходном веществе присутствуют примеси, и при этом примеси включают одно или более из следующих веществ: циклопентадиен, гексан, метилциклопентан, бензол, циклогексен, гептан, метилциклогексан, толуол, этилбензол, фенилацетилен, стирол, нонан, инден, нафталин, метилнафталин, аценафталин и флуорен.6. The method according to claim 5, in which impurities are present in the liquid starting material, and the impurities include one or more of the following substances: cyclopentadiene, hexane, methylcyclopentane, benzene, cyclohexene, heptane, methylcyclohexane, toluene, ethylbenzene, phenylacetylene, styrene , nonane, indene, naphthalene, methylnaphthalene, acenaphthalene and fluorene. 7. Способ по пп.1-6, в котором химическую чистоту жидкого исходного вещества регулируют при помощи операции перегонки, включенной в основное производство.7. The method according to claims 1 to 6, in which the chemical purity of the liquid starting substance is controlled using the distillation operation included in the main production. 8. Способ по п.7, в котором химическую чистоту жидкого исходного вещества регулируют таким образом, что она находится в диапазоне приблизительно 95±5%.8. The method according to claim 7, in which the chemical purity of the liquid starting material is controlled so that it is in the range of approximately 95 ± 5%. 9. Способ по п.7, в котором химическую чистоту жидкого исходного вещества регулируют таким образом, что она находится в диапазоне приблизительно 90±5%, при помощи смешивания химически чистого жидкого исходного вещества с состаренным жидким исходным веществом, содержащим одну или более примесей, соответствующих проведению одного или более циклов уплотнения.9. The method according to claim 7, in which the chemical purity of the liquid starting material is controlled so that it is in the range of about 90 ± 5%, by mixing a chemically pure liquid starting material with an aged liquid starting material containing one or more impurities, corresponding to one or more compaction cycles. 10. Способ по п.1, в котором жидкое исходное вещество содержит органосилан.10. The method according to claim 1, in which the liquid starting substance contains organosilane. 11. Способ по п.10, в котором органосилан выбирают из группы, состоящей из метилтрихлорсилана, диметилдихлорсилана, метилдихлорсилана и трис-н-метиламиносилана.11. The method of claim 10, wherein the organosilane is selected from the group consisting of methyltrichlorosilane, dimethyldichlorosilane, methyldichlorosilane and tris-n-methylaminosilane. 12. Способ по п.10, в котором продукт разложения включает карбид кремния и нитрид кремния.12. The method of claim 10, wherein the decomposition product comprises silicon carbide and silicon nitride. 13. Способ по п.1, в котором жидкое исходное вещество представляет собой смесь органосилана и углеводорода.13. The method according to claim 1, in which the liquid starting substance is a mixture of organosilane and hydrocarbon. 14. Способ по п.12, в котором продукт разложения представляет собой углерод/карбид кремния или углерод/нитрид кремния.14. The method of claim 12, wherein the decomposition product is carbon / silicon carbide or carbon / silicon nitride. 15. Реактор для проведения уплотнения пористых заготовок с использованием матрицы жидкого исходного вещества, включающий:15. A reactor for compacting porous preforms using a matrix of liquid starting material, including: реакционную камеру;reaction chamber; по меньшей мере одно нагревательное устройство, включающее катушки индуктивности, расположенное внутри реакционной камеры;at least one heating device including inductors located inside the reaction chamber; индикатор уровня жидкости для мониторинга расхода жидкого исходного вещества;liquid level indicator for monitoring the flow rate of a liquid source substance; средства добавления жидкого исходного вещества в процессе осуществления уплотнения;means for adding a liquid starting material during compaction; средства продувки реакционной камеры инертным газом;means for purging the reaction chamber with an inert gas; систему извлечения паров, соединенную с реакционной камерой, конструкция и расположение которой позволяет осуществлять конденсацию паров исходного вещества в реакционной камере и возвращать сконденсированное исходное вещество в реакционный сосуд;a vapor recovery system connected to the reaction chamber, the design and arrangement of which allows condensation of the vapors of the starting material in the reaction chamber and returning the condensed starting material to the reaction vessel; выпускную систему, соединяющую систему извлечения паров и средства для продувки с камерой термического окисления; иan exhaust system connecting the vapor recovery system and the purge means to the thermal oxidation chamber; and средства нагнетания давления, предназначенные для поддержания в реакторе давления, составляющего приблизительно от 760 до 780 мм рт.ст. (приблизительно от 1,01·105 до 1,04·105 Па), при проведении операции уплотнения.pressure injection means for maintaining a pressure in the reactor of approximately 760 to 780 mm Hg. (from about 1.01 · 10 5 to 1.04 · 10 5 Pa), during the compaction operation. 16. Способ по п.1, в котором индукционное нагревание погруженного пористого субстрата включает:16. The method according to claim 1, in which induction heating of the immersed porous substrate includes: установку начальных значений частоты и мощности индукционного нагревания, при которых начальные значения частоты и мощности достаточны для создания эффективного количества тепла в области геометрического центра пористого субстрата, достаточного для осуществления пиролиза паров жидкого исходного вещества, предпочтительно в порах, находящихся в области геометрического центра пористого субстрата;setting the initial values of the frequency and power of induction heating at which the initial values of frequency and power are sufficient to create an effective amount of heat in the region of the geometric center of the porous substrate, sufficient to effect pyrolysis of the vapor of the liquid starting material, preferably in pores located in the region of the geometric center of the porous substrate; подачу начальной мощности при начальной частоте, требуемой для индукционного нагревания, достаточного для осуществления уплотнения области геометрического центра пористого субстрата без одновременного уплотнения других частей пористого субстрата;supplying the initial power at the initial frequency required for induction heating, sufficient to densify the region of the geometric center of the porous substrate without simultaneously compressing other parts of the porous substrate; после осуществления уплотнения области геометрического центра пористого субстрата, установление значений подаваемой мощности и частоты таким образом, который позволяет осуществлять последовательное уплотнение внутренних областей пористого субстрата в радиальном направлении от области геометрического центра пористого субстрата к наружных участкам пористого субстрата, иafter densification of the region of the geometric center of the porous substrate, setting the supplied power and frequency in such a way as to sequentially densify the inner regions of the porous substrate in the radial direction from the region of the geometric center of the porous substrate to the outer portions of the porous substrate, and линейное снижение значения мощности до нуля и окончание процесса уплотнения.linear reduction of the power value to zero and the end of the compaction process. 17. Способ по п.1, дополнительно включающий тепловую обработку, производимую после осуществления уплотнения, причем тепловая обработка включает:17. The method according to claim 1, further comprising a heat treatment produced after compaction, wherein the heat treatment includes: полное извлечение жидкого исходного вещества из реакционной камеры;complete recovery of the liquid starting material from the reaction chamber; продувку реакционной камеры инертным газом;purging the reaction chamber with an inert gas; индукционное нагревание уплотненной пористого субстрата в атмосфере инертного газа при температуре, составляющей приблизительно от 1600 до 2400°С, при одновременном поддержании давления, составляющего приблизительно от 760 до 780 мм рт.ст. (приблизительно от 1,01·105 Па до 1,04·105 Па); иinduction heating the densified porous substrate in an inert gas atmosphere at a temperature of about 1600 to 2400 ° C. while maintaining a pressure of about 760 to 780 mm Hg. (approximately 1.01 · 10 5 Pa to 1.04 · 10 5 Pa); and линейное снижение индукционного нагревания до нуля для завершения тепловой обработки. linear reduction of induction heating to zero to complete the heat treatment.
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